CN102531570A - Low-temperature sintering microwave dielectric ceramic material with high Q value and preparation method thereof - Google Patents
Low-temperature sintering microwave dielectric ceramic material with high Q value and preparation method thereof Download PDFInfo
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- CN102531570A CN102531570A CN2011104571573A CN201110457157A CN102531570A CN 102531570 A CN102531570 A CN 102531570A CN 2011104571573 A CN2011104571573 A CN 2011104571573A CN 201110457157 A CN201110457157 A CN 201110457157A CN 102531570 A CN102531570 A CN 102531570A
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Abstract
The invention belongs to the technical field of the material science, in particular to a low-temperature sintering microwave dielectric ceramic material with a high Q value and a preparation method thereof. The low-temperature sintering microwave dielectric ceramic material with a high Q value has the raw material formula composition of Li2(Mg1-xZnx)Ti3O8 and a sintering assistant, wherein x is more than or equal to 0 and less than or equal to 1; and the sintering assistant accounts for 0.5-5wt% of Li2(Mg1-xZnx)Ti3O8 and is one or more of Li2O-B2O3-SiO2 glass powder, ZnO-B2O3-SiO2 glass powder, BaO-O-B2O3-SiO2 glass powder and CuO-Bi2O3-V2O5 sintering powder. The low-temperature sintering microwave dielectric ceramic material provided by the invention has the advantages of low cost, small added sintering dose, high quality factor Qf value, simple preparation technology, good reproducibility and great industrial application value.
Description
Technical field
The invention belongs to materials science field, relate in particular to a kind of high Q value low-temperature sintered microwave dielectric ceramic material and preparation method thereof.
Background technology
Adopt the chip electronic component of LTCC (Low Temperature Co-firing Ceramic is called for short LTCC) fabrication techniques to have characteristics such as miniaturized, integrated level height, high frequency performance and good reliability.In the last thirty years, along with the fast development of Modern wireless communication and mobile communication, the LTCC technology has obtained significant progress.The low-melting metal A g of LTCC Technology Need microwave-medium ceramics and high conductivity, Cu are as interior electrode, and therefore, the low temperature sintering microwave dielectric ceramic materials has become the research focus, have realized Al at present
2O
3, (Mg, Ca) TiO
3, ZnO-TiO
2, Ba
2Ti
9O
20, Li
2O-Nb
2O
5-TiO
2Low-temperature sintering etc. a plurality of material systems.Along with microwave technology towards higher frequency, promptly develop towards millimeter wave and sub-millimeter wave direction, people have higher requirement especially demanding quality factor q value to the dielectric properties of low-temperature sintering microwave medium pottery.
Though most of microwave dielectric ceramic materials have excellent microwave dielectric property, like high Q value, sintering temperature is very high, generally 1200 ~ 1500
oC is the common burning of electrodes such as realization and Ag, Cu, needs to add the sintering temperature that a large amount of low-melting oxide compounds or glass auxiliary agent reduce microwave dielectric ceramic materials usually.The introducing of a large amount of sintering aids often causes the obvious deterioration of ceramic Q value.And adopt the low stupalith of intrinsic sintering temperature to carry out the LTCC investigation of materials is the research focus always.
Summary of the invention
For the introducing that solves a large amount of sintering aids often causes the technological deficiency of the obvious deterioration of ceramic Q value, one object of the present invention is to provide a kind of high Q value low-temperature sintered microwave dielectric ceramic material, and this stupalith successfully reduces to 900 with the sintering temperature of pottery
oBelow the C, keep excellent dielectric properties, especially high Q value simultaneously.Another object of the present invention provides the preparation method of above-mentioned high Q value low-temperature sintered microwave dielectric ceramic material.
In order to realize first above-mentioned technical purpose, the technical scheme below the present invention has adopted:
A kind of high Q value low-temperature sintered microwave dielectric ceramic material, the composition of raw materials of this stupalith consists of: Li
2(Mg
1-xZn
x) Ti
3O
8And sintering aid, wherein 0≤x≤1; Sintering aid accounts for Li
2(Mg
1-xZn
x) Ti
3O
80.5%～5% of massfraction; Sintering aid is Li
2O-B
2O
3-SiO
2Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5In the calcining powder one or more.
As preferably, above-mentioned sintering aid accounts for Li
2(Mg
1-xZn
x) Ti
3O
81%～3% of massfraction.
As preferably, above-mentioned sintering aid is Li
2O-B
2O
3-SiO
2Glass powder, wherein Li
2O-B
2O
3-SiO
2Each component mole percent level is in the glass powder: Li
2O 25%～40%, B
2O
330%～45%, SiO
220%～35%.
As preferably, above-mentioned sintering aid is ZnO-B
2O
3-SiO
2Glass powder, wherein ZnO-B
2O
3-SiO
2Each component mole percent level is in the glass powder: ZnO 30%～70%, B
2O
320%～50%, SiO
210%～30%.
As preferably, above-mentioned sintering aid is BaO-B
2O
3-SiO
2Glass powder, wherein BaO-B
2O
3-SiO
2Each component mole percent level is in the glass powder: BaO20%～60%, B
2O
320%～70%, SiO
25%～25%.
As preferably, above-mentioned sintering aid is CuO-Bi
2O
3-V
2O
5Calcining powder, wherein CuO-Bi
2O
3-V
2O
5Each component molar percentage is CuO:Bi in the calcining powder
2O
3: V
2O
5Equal 1:1:1.
In order to realize second above-mentioned technical purpose, the technical scheme below the present invention has adopted:
A kind of preparation method of above-mentioned high Q value low-temperature sintered microwave dielectric ceramic material, this method may further comprise the steps:
1) presses Li
2(Mg
1-xZn
x) Ti
3O
8Stoichiometric weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol～1.5 and add ethanol, adopt behind material by wet type mixing 16～24h in 70～90 ℃ of oven dry; The compound of oven dry is crossed 40 mesh sieves, and the alumina crucible of packing into is calcined 2～4h down at 750～900 ℃; Synthetic principal crystalline phase, subsequent use after grinding as ceramic base-material;
2) sintering aid Li
2O-B
2O
3-SiO
2-CaO-Al
2O
3Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5The calcining powder is synthetic;
3) with the Li for preparing
2(Mg
1-xZn
x) Ti
3O
8Pottery base-material and Li
2O-B
2O
3-SiO
2Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5One or more sintering aids in the calcining powder mix by proportioning; Select ZrO for use
2Abrading-ball is pressed the weight ratio 1:1 of compound and absolute ethyl alcohol～1.5 and is added ethanol, adopts behind material by wet type mixing 16～24h in 70～90 ℃ of oven dry; Add 5 wt%～8wt% poly (vinyl alcohol) binder granulation; Press down at 80～120Mpa pressure and to process diameter 20mm, the nahlock of thickness 10mm is at 850～950 ℃ of sintering; Insulation 2～4h promptly obtains described high Q value low-temperature sintered microwave dielectric ceramic material.
As preferably, above-mentioned Li
2O-B
2O
3-SiO
2-CaO-Al
2O
3The preparation method of glass powder is following:
1) with Li
2CO
3, B
2O
3, SiO
2By following molar content proportioning: Li
2CO
325～40%, B
2O
330～45%, SiO
220～35%, take by weighing the Li of oven dry
2CO
3, B
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1000 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 30min, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
As preferably, above-mentioned ZnO-B
2O
3-SiO
2The preparation method of glass powder is following:
1) with ZnO, B
2O
3, SiO
2Press following molar content proportioning: ZnO 30～70%, B
2O
320～50%, SiO
210～30%, take by weighing ZnO, the B of oven dry
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1100 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 40min, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
As preferably, above-mentioned BaO-B
2O
3-SiO
2The preparation method of glass powder is following:
1) with BaO, B
2O
3, SiO
2By following molar content proportioning: BaCO
320～60%, B
2O
320～70%, SiO
25～25%, take by weighing BaO, the B of oven dry
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1300 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 1h, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
As preferably, above-mentioned CuO-Bi
2O
3-V
2O
5The preparation method of calcining powder is following: with CuO, Bi
2O
3, V
2O
5Take by weighing CuO, the Bi of oven dry by the 1:1:1 mol ratio
2O
3And V
2O
5, select ZrO for use
2Abrading-ball, weight ratio 1:1～1.5 of pressing compound and absolute ethyl alcohol add ethanol, in 80 ℃ of oven dry, the compound of oven dry are crossed 40 mesh sieves behind the employing material by wet type mixing 16-24h, and the alumina crucible of packing into is calcined 3h down at 600 ℃, and is subsequent use after grinding.
The present invention adopts the Li that sintering temperature is low, dielectric properties are excellent
2(Mg, Zn) Ti
3O
8System is as body material, through introducing a small amount of Li
2O-B
2O
3-SiO
2Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5Sintering aids such as calcining powder successfully reduce to 900 with the sintering temperature of pottery
oBelow the C, and have the excellent microwave dielectric properties: specific inductivity
ε r =21 ~ 27,
Q * f=8000 ~ 28000GHz, frequency-temperature coefficient
τ f Adjustable.Can be used for preparing novel chip multilayer microwave devices such as wave filter, resonator, duplexer, Ba Lun.Low-temperature sintered microwave dielectric ceramic material provided by the invention is with low cost, and interpolation sintering aid amount is few, has high quality factor q f value, and preparation technology is simple, favorable reproducibility, so the present invention has great industrial application value.
Embodiment
The present invention will be described below in conjunction with embodiment.
Embodiment 1
Press Li
2(Mg
0.7Zn
0.3) Ti
3O
8Stoichiometry weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol ~ 1.5 and add ethanol, adopt behind the material by wet type mixing 16-24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is at 750-900
oC is calcining 2-4h down, and synthetic principal crystalline phase is subsequent use as ceramic base-material after grinding.
With Li
2CO
3, B
2O
3, SiO
2By following molar content proportioning: Li
2CO
330%, B
2O
340%, SiO
230%, take by weighing the Li of oven dry
2CO
3, H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h, then with the mixed powder corundum crucible of packing into, with 5
oThe temperature rise rate of C/min is heated to 1000
oC behind the insulation homogenizing 30min, pours quenching in the water into.With the frit that obtains 120
oZrO is still used in the C oven dry
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h.The glass powder that obtains is crossed 100 mesh sieves, and is for use.
Li with 100g
2(Mg
0.7Zn
0.3) Ti
3O
8The Li of pottery base-material and 3g
2O-B
2O
3-SiO
2Glass powder mixes, and formula number is L1.Select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, behind the batch mixing 20h in 80
oThe C oven dry adds the granulation of 5wt% Z 150PH (PVA) tackiness agent, presses down at 100Mpa pressure and processes diameter 20mm, and the nahlock of thickness 10mm is 930
oThe C sintering, insulation 3h.After the sample surfaces of preparation carries out grinding and polishing with silicon carbide, measure dielectric properties.
Embodiment 2
Press Li
2(Mg
0.7Zn
0.3) Ti
3O
8Stoichiometry weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol ~ 1.5 and add ethanol, adopt behind the material by wet type mixing 16-24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is at 750-900
oC is calcining 2-4h down, and synthetic principal crystalline phase is subsequent use as ceramic base-material after grinding.
With ZnO, B
2O
3, SiO
2Press following molar content proportioning: ZnO 60%, B
2O
330%, SiO
210%, take by weighing ZnO, the H of oven dry
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h, then with the mixed powder corundum crucible of packing into, with 5
oThe temperature rise rate of C/min is heated to 1100
oC behind the insulation homogenizing 40min, pours quenching in the water into.With the frit that obtains 120
oZrO is still used in the C oven dry
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h.The glass powder that obtains is crossed 100 mesh sieves, and is for use.
Li with 100g
2(Mg
0.7Zn
0.3) Ti
3O
8The ZnO-B of pottery base-material and 1g
2O
3-SiO
2Glass powder mixes, and formula number is L2.Select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, behind the batch mixing 20h in 80
oThe C oven dry adds the granulation of 5wt% Z 150PH (PVA) tackiness agent, presses down at 100Mpa pressure and processes diameter 20mm, and the nahlock of thickness 10mm is 880
oThe C sintering, insulation 3h.After the sample surfaces of preparation carries out grinding and polishing with silicon carbide, measure dielectric properties.
Embodiment 3
Press Li
2(Mg
0.7Zn
0.3) Ti
3O
8Stoichiometry weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol ~ 1.5 and add ethanol, adopt behind the material by wet type mixing 16-24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is at 750-900
oC is calcining 2-4h down, and synthetic principal crystalline phase is subsequent use as ceramic base-material after grinding.
With ZnO, B
2O
3, SiO
2Press a mole percentage composition proportioning: ZnO 60%, B
2O
330%, SiO
210%, take by weighing ZnO, the H of oven dry
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h, then with the mixed powder corundum crucible of packing into, with 5
oThe temperature rise rate of C/min is heated to 1100
oC behind the insulation homogenizing 40min, pours quenching in the water into.With the frit that obtains 120
oZrO is still used in the C oven dry
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h.The glass powder that obtains is crossed 100 mesh sieves, and is for use.
Li with 100g
2(Mg
0.7Zn
0.3) Ti
3O
8The ZnO-B of pottery base-material and 3g
2O
3-SiO
2Glass powder mixes, and formula number is L3.Select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, behind the batch mixing 20h in 80
oThe C oven dry adds the granulation of 5wt% Z 150PH (PVA) tackiness agent, presses down at 100Mpa pressure and processes diameter 20mm, and the nahlock of thickness 10mm is 880
oThe C sintering, insulation 3h.After the sample surfaces of preparation carries out grinding and polishing with silicon carbide, measure dielectric properties.
Embodiment 4
Press Li
2(Mg
0.7Zn
0.3) Ti
3O
8Stoichiometry weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol ~ 1.5 and add ethanol, adopt behind the material by wet type mixing 16-24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is at 750-900
oC is calcining 2-4h down, and synthetic principal crystalline phase is subsequent use as ceramic base-material after grinding.
With BaO, B
2O
3, SiO
2Press a mole percentage composition proportioning: BaO 30%, B
2O
360%, SiO
210%, take by weighing BaO, the H of oven dry
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h, then with the mixed powder corundum crucible of packing into, with 5
oThe temperature rise rate of C/min is heated to 1300
oC behind the insulation homogenizing 1h, pours quenching in the water into.With the frit that obtains 120
oZrO is still used in the C oven dry
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h.The glass powder that obtains is crossed 100 mesh sieves, and is for use.
Li with 100g
2(Mg
0.7Zn
0.3) Ti
3O
8The BaO-B of pottery base-material and 3g
2O
3-SiO
2Glass powder mixes, and formula number is L4.Select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, behind the batch mixing 20h in 80
oThe C oven dry adds the granulation of 5wt% Z 150PH (PVA) tackiness agent, presses down at 100Mpa pressure and processes diameter 20mm, and the nahlock of thickness 10mm is 880
oThe C sintering, insulation 3h.After the sample surfaces of preparation carries out grinding and polishing with silicon carbide, measure dielectric properties.
Embodiment 5
Press Li
2(Mg
0.7Zn
0.3) Ti
3O
8Stoichiometry weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol ~ 1.5 and add ethanol, adopt behind the material by wet type mixing 16-24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is at 750-900
oC is calcining 2-4h down, and synthetic principal crystalline phase is subsequent use as ceramic base-material after grinding.
With CuO, Bi
2O
3, V
2O
5Take by weighing CuO, the Bi of oven dry by the 1:1:1 mol ratio
2O
3And V
2O
5, select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, adopts behind the material by wet type mixing 24h in 80
oThe C oven dry is crossed 40 mesh sieves with the compound of oven dry, and the alumina crucible of packing into is 600
oC is calcining 3h down, and is subsequent use after grinding.
Li with 100g
2(Mg
0.7Zn
0.3) Ti
3O
8The CuO-Bi of pottery base-material and 3g
2O
3-V
2O
5The calcining powder mixes, and formula number is L5.Select ZrO for use
2Abrading-ball, the weight ratio 1:1.5 that presses compound and absolute ethyl alcohol adds ethanol, behind the batch mixing 20h in 80
oThe C oven dry adds the granulation of 5wt% Z 150PH (PVA) tackiness agent, presses down at 100Mpa pressure and processes diameter 20mm, and the nahlock of thickness 10mm is 900
oThe C sintering, insulation 3h.After the sample surfaces of preparation carries out grinding and polishing with silicon carbide, measure dielectric properties.
Table 1 is the prescription and the dielectric properties of embodiment 1 to 6 correspondence.Wherein, dielectric properties are measured and are adopted Agilent 8719ET network analyzer, measure specific inductivity according to the Hakki-Coleman Resonant-cavity Method
ε r With quality factor q f, frequency-temperature coefficient
τ f In 25～80 ℃ of TRs, measure, and by formula:
τ f =(f
80-f
25)/(f
25* 55) calculate, wherein f
80And f
25Be respectively 80
oC and 25
oResonance mid-frequency under the C.
Table 1 ceramic composition and dielectric properties (test frequency f=4.4GHz)
| Formula number | Sintering aid | Content (wt%) | Sintering temperature oC | ε r | Qf(GHz) | τ f(ppm/ oC) |
| L1 | Li 2O-B 2O 3-SiO 2Glass powder | 3 | 930 | 24.5 | 23280 | -3.5 |
| L2 | ZnO-B 2O 3-SiO 2Glass powder | 1 | 880 | 23.7 | 24000 | -1.3 |
| L3 | ZnO-B 2O 3-SiO 2Glass powder | 3 | 880 | 23.7 | 26460 | -7.1 |
| L4 | BaO-B 2O 3-SiO 2Glass powder | 3 | 880 | 24.7 | 17950 | -7.9 |
| L5 | CuO-Bi 2O 3-V 2O 5The calcining powder | 3 | 900 | 26.2 | 8019 | -5.5 |
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these contents.Prove according to applicant's lot of experiment results,, all can reach the object of the invention in the scope that claims of the present invention proposed.
Claims (10)
1. one kind high Q value low-temperature sintered microwave dielectric ceramic material is characterized in that the composition of raw materials of this stupalith consists of:
Li
2(Mg
1-xZn
x) Ti
3O
8And sintering aid, wherein 0≤x≤1;
Sintering aid accounts for Li
2(Mg
1-xZn
x) Ti
3O
80.5%～5% of massfraction; Account for Li as the described sintering aid of optimal way
2(Mg
1-xZn
x) Ti
3O
81%～3% of massfraction;
Sintering aid is Li
2O-B
2O
3-SiO
2Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5In the calcining powder one or more.
2. a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 1, it is characterized in that: sintering aid is Li
2O-B
2O
3-SiO
2Glass powder, wherein Li
2O-B
2O
3-SiO
2Each component mole percent level is in the glass powder: Li
2O 25%～40%, B
2O
330%～45%, SiO
220%～35%.
3. a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 1, it is characterized in that: sintering aid is ZnO-B
2O
3-SiO
2Glass powder, wherein ZnO-B
2O
3-SiO
2Each component mole percent level is in the glass powder: ZnO 30%～70%, B
2O
320%～50%, SiO
210%～30%.
4. a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 1, it is characterized in that: sintering aid is BaO-B
2O
3-SiO
2Glass powder, wherein BaO-B
2O
3-SiO
2Each component mole percent level is in the glass powder: BaO20%～60%, B
2O
320%～70%, SiO
25%～25%.
5. a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 1, it is characterized in that: sintering aid is CuO-Bi
2O
3-V
2O
5Calcining powder, wherein CuO-Bi
2O
3-V
2O
5Each component molar percentage is CuO:Bi in the calcining powder
2O
3: V
2O
5Equal 1:1:1.
6. preparation method who prepares the described high Q value low-temperature sintered microwave dielectric ceramic material of claim 1 is characterized in that this method may further comprise the steps:
1) presses Li
2(Mg
1-xZn
x) Ti
3O
8Stoichiometric weighing major ingredient Li
2CO
3, MgO, ZnO and TiO
2, press the weight ratio 1:1 of compound and absolute ethyl alcohol～1.5 and add ethanol, adopt behind material by wet type mixing 16～24h in 70～90 ℃ of oven dry; The compound of oven dry is crossed 40 mesh sieves, and the alumina crucible of packing into is calcined 2～4h down at 750～900 ℃; Synthetic principal crystalline phase, subsequent use after grinding as ceramic base-material;
2) sintering aid Li
2O-B
2O
3-SiO
2-CaO-Al
2O
3Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5The calcining powder is synthetic;
3) with the Li for preparing
2(Mg
1-xZn
x) Ti
3O
8Pottery base-material and Li
2O-B
2O
3-SiO
2Glass powder, ZnO-B
2O
3-SiO
2Glass powder, BaO-B
2O
3-SiO
2Glass powder and CuO-Bi
2O
3-V
2O
5One or more sintering aids in the calcining powder mix by proportioning; Select ZrO for use
2Abrading-ball is pressed the weight ratio 1:1 of compound and absolute ethyl alcohol～1.5 and is added ethanol, adopts behind material by wet type mixing 16～24h in 70～90 ℃ of oven dry; Add 5 wt%～8wt% poly (vinyl alcohol) binder granulation; Press down at 80～120Mpa pressure and to process diameter 20mm, the nahlock of thickness 10mm is at 850～950 ℃ of sintering; Insulation 2～4h promptly obtains described high Q value low-temperature sintered microwave dielectric ceramic material.
7. the preparation method of a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 6 is characterized in that
Li
2O-B
2O
3-SiO
2-CaO-Al
2O
3The preparation method of glass powder is following:
1) with Li
2CO
3, B
2O
3, SiO
2By following molar content proportioning: Li
2CO
325～40%, B
2O
330～45%, SiO
220～35%, take by weighing the Li of oven dry
2CO
3, B
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1000 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 30min, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
8. the preparation method of a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 6 is characterized in that
ZnO-B
2O
3-SiO
2The preparation method of glass powder is following:
1) with ZnO, B
2O
3, SiO
2Press following molar content proportioning: ZnO 30～70%, B
2O
320～50%, SiO
210～30%, take by weighing ZnO, the B of oven dry
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1100 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 40min, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
9. the preparation method of a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 6 is characterized in that BaO-B
2O
3-SiO
2The preparation method of glass powder is following:
1) with BaO, B
2O
3, SiO
2By following molar content proportioning: BaCO
320～60%, B
2O
320～70%, SiO
25～25%, take by weighing BaO, the B of oven dry
2O
3Or H
3BO
3And SiO
2, select ZrO for use
2Abrading-ball adopts dry method batch mixing 1h;
2) then with the mixed powder corundum crucible of packing into, be heated to 1300 ℃ with the temperature rise rate of 5 ℃/min, behind the insulation homogenizing 1h, pour quenching in the water into;
3) with the frit that obtains 120 ℃ of oven dry, still use ZrO
2Abrading-ball adopts the dry method rolling ball milling to pulverize 24h; The glass powder that obtains is crossed 100 mesh sieves, and is for use.
10. the preparation method of a kind of high Q value low-temperature sintered microwave dielectric ceramic material according to claim 6 is characterized in that CuO-Bi
2O
3-V
2O
5The preparation method of calcining powder is following: with CuO, Bi
2O
3, V
2O
5Take by weighing CuO, the Bi of oven dry by the 1:1:1 mol ratio
2O
3And V
2O
5, select ZrO for use
2Abrading-ball, weight ratio 1:1～1.5 of pressing compound and absolute ethyl alcohol add ethanol, in 80 ℃ of oven dry, the compound of oven dry are crossed 40 mesh sieves behind the employing material by wet type mixing 16-24h, and the alumina crucible of packing into is calcined 3h down at 600 ℃, and is subsequent use after grinding.
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